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EUROPEAN PHARMACOPOEIA 5.

Fusidic acid

IMPURITIES

A. 2-chloro-4-[(furan-2-ylmethyl)amino]-5-sulphamoylbenzoic acid,

B. R1 = Cl, R2 = SO2-NH2 : 2,4-dichloro-5-sulphamoylbenzoic acid, TESTS C. R1 = NH2, R2 = SO2-NH2 : 2-amino-4-chloro-5Related substances. Examine by liquid chromatography sulphamoylbenzoic acid, (2.2.29). E. R1 = Cl, R2 = H : 2,4-dichlorobenzoic acid, Test solution. Dissolve 50 mg of the substance to be examined in the mobile phase and dilute to 10.0 ml with the mobile phase. Reference solution (a). Dissolve 5 mg of 3-ketofusidic acid CRS in 5 ml of the mobile phase. To 1.0 ml of this solution add 0.20 ml of the test solution and dilute to 20.0 ml with the mobile phase. Reference solution (b). Dilute 20 l of the test solution to D. 2,4-bis[(furan-2-ylmethyl)amino]-5-sulphamoylbenzoic 100.0 ml with the mobile phase. acid. The chromatographic procedure may be carried out using : 01/2005:0798 a steel column 0.125 m to 0.15 m long and 4 mm to 5 mm in internal diameter packed with octadecylsilyl silica gel for chromatography R (5 m), FUSIDIC ACID as mobile phase at a flow rate of 2 ml/min a mixture of 10 volumes of methanol R, 20 volumes of a 10 g/l Acidum fusidicum solution of phosphoric acid R, 20 volumes of water R and 50 volumes of acetonitrile R, as detector a spectrophotometer set at 235 nm, a 20 l loop injector. Continue the chromatography for at least 3.5 times the retention time of the principal peak. In the chromatogram obtained with the test solution, the sum of the areas of the peaks, apart from the principal peak and the solvent peak, is not greater than twice the area of the peak corresponding to fusidic acid in the chromatogram obtained with reference solution (a) (2.0 per cent). Disregard any peak with an area less than that of the principal peak in the chromatogram C31H48O6, 1/2H2O Mr 525.7 obtained with reference solution (b). The test is not valid unless : the resolution between the peaks corresponding DEFINITION to 3-ketofusidic acid and fusidic acid in the chromatogram Fusidic acid is ent-(17Z)-16-(acetyloxy)-3,11-dihydroxy-4, obtained with reference solution (a) is at least 2.5 ; the 8,14-trimethyl-18-nor-5,10-cholesta-17(20),24-dien-21-oic principal peak in the chromatogram obtained with reference acid, an antimicrobial substance produced by the growth solution (b) has a signal-to-noise ratio of at least 3. of certain strains of Fusidium coccineum or by any other Water (2.5.12) : 1.4 per cent to 2.0 per cent, determined on means. It contains not less than 97.5 per cent and not more 0.50 g by the semi-micro determination of water. than the equivalent of 101.0 per cent of C31H48O6, calculated Sulphated ash (2.4.14). Not more than 0.2 per cent, with reference to the anhydrous substance. determined on 1.0 g. CHARACTERS ASSAY A white or almost white, crystalline powder, practically Dissolve 0.500 g in 10 ml of alcohol R. Add 0.5 ml of insoluble in water, freely soluble in alcohol. phenolphthalein solution R. Titrate with 0.1 M sodium IDENTIFICATION hydroxide until a pink colour is obtained. A. Examine by infrared absorption spectrophotometry 1 ml of 0.1 M sodium hydroxide is equivalent to 51.67 mg of (2.2.24), comparing with the spectrum obtained with the C H O . 31 48 6 Ph. Eur. reference spectrum of fusidic acid. STORAGE B. Examine by thin-layer chromatography (2.2.27), using silica gel HF254 R as the coating substance. Store protected from light, at a temperature of 2 C to 8 C. General Notices (1) apply to all monographs and other texts 1645

Test solution. Dissolve 20 mg of the substance to be examined in methanol R and dilute to 10 ml with the same solvent. Reference solution. Dissolve 24 mg of diethanolamine fusidate CRS in methanol R and dilute to 10 ml with the same solvent. Apply to the plate 10 l of each solution. Develop over a path of 15 cm using a mixture of 2.5 volumes of methanol R, 10 volumes of glacial acetic acid R, 10 volumes of cyclohexane R and 80 volumes of chloroform R. Dry the plate in a current of hot air. Examine in ultraviolet light at 254 nm. The principal spot in the chromatogram obtained with the test solution is similar in position and size to the principal spot in the chromatogram obtained with the reference solution.

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